Patent US4402928A successfully refreshed from Google Patents.
US4402928A
Expired / Lapsed
US
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Carbon fiber production using high pressure treatment of a precursor material
Assignee: BP Corp North America Inc
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Filing: 1981-03-27
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Granted: 1983-09-06
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Expires: 2001-03-27
Abstract
Abstract A process for producing a carbon fiber includes the steps of heat treating a selected precursor material under high pressure, thereafter solvent extracting the treated precursor material to obtain mesophase pitch, spinning the mesophase pitch into at least one pitch fiber, thermosetting the pitch fiber, and carbonizing the pitch fiber to obtain the carbon fiber.
Inventors
- 👤 Irwin C. Lewis
- 👤 Arthur W. Moore
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 16:32
CPC Classifications
D; D01; D01F; D01F9/00; D01F9/08; D01F9/12; D01F9/14; D01F9/32; D01F9/322; D01F9/145
Claims Analysis
Total Claims: 35
Claim 1
Independent Claim
194 words
A process for producing carbon fiber, comprising the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, and aromatic hydrocarbons; subjecting the material to a thermal-pressure treatment as a batch treatment at a temperature from about 400° C. to about 475° C. and at a pressure from about 750 psig to about 1500 psig to obtain a precursor pitch, the soaking volume factor of said treatment being at least 0.4. solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular weight distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is a mesophase pitch containing at least 70% by weight mesophase; spinning the mesophase pitch into at least one pitch fiber; and converting the pitch fiber into the carbon fiber.
Claim 2
Dependent Claim
194 words
A process for producing carbon fiber, comprising the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, and aromatic hydrocarbons; subjecting the material to a thermal-pressure treatment as a batch treatment at a temperature from about 400° C. to about 475° C. and at a pressure from about 750 psig to about 1500 psig to obtain a precursor pitch, the soaking volume factor of said treatment being at least 0.4. solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular weight distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is a mesophase pitch containing at least 70% by weight mesophase; spinning the mesophase pitch into at least one pitch fiber; and converting the pitch fiber into the carbon fiber.
Claim 3
Dependent Claim
21 words
The process of claim 1, wherein the soaking volume factor for the thermal-pressure treatment is from about 0.4 to about 8.6.
Claim 4
Dependent Claim
27 words
The process of claim 2, wherein the thermal-pressure treatment is continued until the Conradson carbon content of the precursor pitch is from about 20% to about 65%.
Claim 5
Dependent Claim
15 words
The process of claim 3, wherein the Conradson carbon content is at least about 30%.
Claim 6
Dependent Claim
17 words
The process of claim 3, wherein the thermal-pressure treatment is carried out with the material being agitated.
Claim 7
Dependent Claim
14 words
The process of claim 5, wherein the agitation is in the form of stirring.
Claim 8
Dependent Claim
21 words
The process of claim 3, further comprising filtering the precursor pitch prior to the solvent extracting step to remove infusible solids.
Claim 9
Dependent Claim
20 words
The process of claim 3, further comprising distilling the precursor pitch to raise its softening point to a predetermined temperature.
Claim 10
Dependent Claim
14 words
The process of claim 8, wherein the temperature is at least about 120° C.
Claim 11
Dependent Claim
26 words
The process of claim 8, wherein the distilling is carried out to raise the Conradson carbon content of the precursor pitch to at least about 40%.
Claim 12
Dependent Claim
191 words
A process for producing a carbon fiber, comprising the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, and aromatic hydrocarbons; subjecting the material to a continuous treatment at a temperature from about 420° C. to about 550° C. and at a pressure from about 750 psig to about 1500 psig to produce a precursor pitch, the soaking volume factor of said treatment being at least 0.4; solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is a mesophase pitch containing at least about 70% by weight mesophase; spinning the mesophase pitch into at least one pitch fiber; and converting the pitch fiber into the carbon fiber.
Claim 13
Dependent Claim
191 words
A process for producing a carbon fiber, comprising the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, and aromatic hydrocarbons; subjecting the material to a continuous treatment at a temperature from about 420° C. to about 550° C. and at a pressure from about 750 psig to about 1500 psig to produce a precursor pitch, the soaking volume factor of said treatment being at least 0.4; solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is a mesophase pitch containing at least about 70% by weight mesophase; spinning the mesophase pitch into at least one pitch fiber; and converting the pitch fiber into the carbon fiber.
Claim 14
Dependent Claim
21 words
The process of claim 11, wherein the soaking volume factor for the continuous treatment is from about 0.4 to about 2.6.
Claim 15
Dependent Claim
28 words
The process of claim 11, wherein the continuous treatment is carried out until the Conradson carbon content of the precursor pitch is from about 5% to about 65%.
Claim 16
Dependent Claim
15 words
The process of claim 13, wherein the Conradson carbon content is at least about 10%.
Claim 17
Dependent Claim
20 words
The process of claim 13, further comprising distilling the precursor pitch to raise its softening point to a predetermined temperature.
Claim 18
Dependent Claim
27 words
The process of claim 15, wherein the distilling step is carried out to raise the Conradson carbon content of the precursor pitch to at least about 40%.
Claim 19
Dependent Claim
176 words
Process for producing a mesophase pitch comprising the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, and aromatic hydrocarbons; subjecting the material to a thermal-pressure treatment as a batch treatment at a temperature from about 400° C. to about 475° C. and at a pressure from about 750 psig to about 1500 psig to obtain a precursor pitch, the soaking volume factor of said treatment being at least 0.4; and solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular weight distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is the mesophase pitch containing at least 70% by weight mesophase.
Claim 20
Dependent Claim
176 words
Process for producing a mesophase pitch comprising the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, and aromatic hydrocarbons; subjecting the material to a thermal-pressure treatment as a batch treatment at a temperature from about 400° C. to about 475° C. and at a pressure from about 750 psig to about 1500 psig to obtain a precursor pitch, the soaking volume factor of said treatment being at least 0.4; and solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular weight distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is the mesophase pitch containing at least 70% by weight mesophase.
Claim 21
Dependent Claim
21 words
The process of claim 17, wherein the soaking volume factor for the thermal-pressure treatment is from about 0.4 to about 8.6.
Claim 22
Dependent Claim
27 words
The process of claim 18, wherein the thermal-pressure treatment is continued until the Conradson carbon content of the precursor pitch is from about 20% to about 65%.
Claim 23
Dependent Claim
15 words
The process of claim 19, wherein the Conradson carbon content is at least about 30%.
Claim 24
Dependent Claim
17 words
The process of claim 19, wherein the thermal-pressure treatment is carried out with the material being agitated.
Claim 25
Dependent Claim
14 words
The process of claim 21, wherein the agitation is in the form of stirring.
Claim 26
Dependent Claim
20 words
The process of claim 20, further comprising distilling the precursor pitch to raise its softening point to a predetermined temperature.
Claim 27
Dependent Claim
14 words
The process of claim 23, wherein the temperature is at least about 120° C.
Claim 28
Dependent Claim
26 words
The process of claim 23, wherein the distilling is carried out to raise the Conradson carbon content of the precursor pitch to at least about 40%.
Claim 29
Dependent Claim
173 words
A process for producing a mesophase pitch, comprising the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, and aromatic hydrocarbons; subjecting the material to a continuous treatment at a temperature from about 420° C. to about 550° C. and at a pressure from about 750 psig to about 1500 psig to produce a precursor pitch, the soaking volume factor of said treatment being at least 0.4; and solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is the mesophase pitch containing at least about 70% by weight mesophase.
Claim 30
Dependent Claim
173 words
A process for producing a mesophase pitch, comprising the steps of: selecting a precursor material from the group consisting of ethylene tars, ethylene tar distillates, gas oils derived from petroleum refining, gas oils derived from petroleum coking, and aromatic hydrocarbons; subjecting the material to a continuous treatment at a temperature from about 420° C. to about 550° C. and at a pressure from about 750 psig to about 1500 psig to produce a precursor pitch, the soaking volume factor of said treatment being at least 0.4; and solvent extracting the precursor pitch until there is obtained an insoluble portion having a molecular distribution wherein at least about 75% of the molecules have a molecular weight in the range of from about 600 to about 1300, less than about 10% of the molecules have a molecular weight less than about 600, and less than about 15% of the molecules have a molecular weight of more than about 1300; whereby the insoluble portion is the mesophase pitch containing at least about 70% by weight mesophase.
Claim 31
Dependent Claim
21 words
The process of claim 26, wherein the soaking volume factor for the continuous treatment is from about 0.4 to about 2.6.
Claim 32
Dependent Claim
28 words
The process of claim 26, wherein the continuous treatment is carried out until the Conradson carbon content of the precursor pitch is from about 5% to about 65%.
Claim 33
Dependent Claim
15 words
The process of claim 28, wherein the Conradson carbon content is at least about 10%.
Claim 34
Dependent Claim
20 words
The process of claim 28, further comprising distilling the precursor pitch to raise its softening point to a predetermined temperature.
Claim 35
Dependent Claim
27 words
The process of claim 30, wherein the distilling step is carried out to raise the Conradson carbon content of the precursor pitch to at least about 40%.
References Cited (Backward Citations)
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1986-09-05 | 1987-03-07 | 1987-09-06 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1990-09-05 | 1991-03-07 | 1991-09-06 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1994-09-05 | 1995-03-07 | 1995-09-06 | $7700.00 | Window Closed / Lapsed |